CN110029258B - High-strength and high-toughness wrought magnesium alloy and preparation method thereof - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/002—Castings of light metals
- B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
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- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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Abstract
The invention relates to a high-strength and high-toughness wrought magnesium alloy and a preparation method thereof. The invention overcomes the defects of the prior art, and compared with the prior art, the wrought magnesium alloy prepared by the invention has the advantages of simple process, strong controllability and more excellent comprehensive mechanical property.
Description
Technical Field
The invention relates to the technical field of alloy material preparation, in particular to a high-strength and high-toughness wrought magnesium alloy and a preparation method thereof.
Background
The magnesium alloy is used as the lightest commercial metal structure material, has the characteristics of minimum density, higher specific strength and specific stiffness, excellent damping performance, good machining performance and the like, and has great application potential in the fields of automobiles, aerospace, medical treatment and the like.
At present, although Mg-Al-Zn, Mg-Zn-Zr series and other magnesium alloys are primarily applied in industry, the mechanical property and the processing property of the magnesium alloys can not meet the requirement of rapid development of the industry. Therefore, microalloying and/or alloying methods are being used to further improve and enhance the mechanical properties and processability of these magnesium alloy systems.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing the high-strength and high-toughness wrought magnesium alloy and the preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a high-strength-toughness wrought magnesium alloy is prepared by adding microalloying elements Zr, Nd and Sr on the basis of a commonly used AZ80 magnesium alloy through a composite treatment method, wherein the alloy comprises the following components in percentage by weight: 7.8 to 9.2 percent of AlAl, 0.2 to 0.8 percent of Zn0.15 to 0.5 percent of Mn0.3 to 1 percent of Zr0.3 to 1 percent of Nd0.1 to 0.5 percent of Sr0.1 to 0.5 percent of impurity elements Si, Fe, Ni and Cu, the total content is less than 0.08 percent, and the balance of Mg.
A preparation method of high-strength and high-toughness wrought magnesium alloy comprises the following steps:
(1) taking a steel crucible, cleaning the steel crucible, heating the steel crucible to 200 ℃, coating the surface of the steel crucible with a mixed solution of talcum powder, water glass and water for three times, coating the surface of the steel crucible with a mixed solution of ZnO, water glass and water for three times until the surface of the steel crucible is not exposed to avoid the pollution of Fe element, and putting the steel crucible back into a heating furnace to keep the temperature for 20 minutes after each coating;
(2) preheating the coated crucible to 520 ℃, putting the magnesium block preheated to 200 ℃ into the crucible, scattering a covering agent on the surface of the magnesium block, introducing argon to the opening of the crucible for gas protection, heating the crucible to 700 ℃, preserving the temperature for 30 minutes, and waiting for the magnesium block to be melted into a body state;
(3) after the magnesium block is melted, rapidly removing slag according to the oxidation and impurity conditions on the surface of the solution, then sequentially adding pure zinc, pure aluminum, pure strontium, Mg-Zr intermediate alloy, Mg-Nd intermediate alloy and MnCl2 particles into the magnesium alloy solution according to the raw material proportion, fully stirring, uniformly scattering a covering agent on the surface of the solution after stirring, and preserving heat for 30 minutes at 700 ℃;
(4) after heat preservation, the furnace temperature is raised to 730 ℃ for refining, a refining agent with the total weight fraction of 1.5 percent is added into the solution, the mixture is fully stirred for 10 minutes, and then the temperature is preserved for 30 minutes at 730 ℃;
(5) cooling the furnace to 680 ℃ after heat preservation, and pouring the furnace into a metal mold which is preserved at 200 ℃ in advance for cooling and solidification;
(6) carrying out homogenizing annealing on the magnesium alloy ingot at 400 ℃, keeping the temperature for 12 hours, machining the blank into a required size after homogenizing annealing, and peeling;
(7) preheating the machined blank to 420 ℃, putting the blank on an extruder for extrusion forming, wherein the preheating temperature of an extrusion cylinder is 400 ℃, the extrusion temperature is 440 ℃, and the extrusion ratio is 25:1, extruding at the speed of 3.5m/min, and cooling the obtained section bar to room temperature in air;
(8) the obtained magnesium alloy section is subjected to solution treatment for 2 hours at 380 ℃ and aging treatment for 18 hours at 170 ℃, and finally the high-strength and high-toughness magnesium alloy section is prepared.
Further, in the step (3), the raw materials have purities of pure magnesium blocks (99.9%), pure zinc blocks (99.9%), pure aluminum blocks (99.9%), pure strontium blocks (99.9%) and MnCl2 (99.9%).
Further, the mixed solution of the talcum powder, the water glass and the water used in the step (1) comprises the following components in a volume ratio of 25: 6: 69.
further, the volume ratio of the components of the mixed liquid of ZnO, water glass and water used in the step (1) is 22: 6: 72.
further, the covering agent used in the step (2) and the step (3) comprises the following components in percentage by weight: CaCl 2: BaCl 2: NaCl 52: 28: 17: 3.
further, the refining agent used in the step (4) comprises the following components in percentage by weight: CaCl 2: BaCl 2: NaCl: CaF2 ═ 50: 27: 16: 2: 5.
further, the MnCl2 used in the step (3) is granular, and the diameter of the granules is 1-3 mm.
Note that: the protective gas is adjusted in real time according to the actual burning loss condition in the smelting process. The slag skimming treatment is carried out according to the actual situation of smelting, and the slag skimming treatment requirement is rapid.
The invention has the following advantages: the alloy is prepared by heating a pure magnesium ingot to be molten under the protective atmosphere, adding alloying elements, refining and casting the alloy into an ingot after the alloying elements are dissolved, carrying out homogenization annealing on the obtained as-cast magnesium alloy, and then carrying out hot extrusion and solution aging treatment on the as-cast magnesium alloy.
The invention has the beneficial effects that the high-strength and high-toughness wrought magnesium alloy prepared by the composite treatment method has higher strength and good ductility, further improves and enhances the comprehensive mechanical property and the processing property of AZ80, and has yield strength of more than 280MPa, tensile strength of more than 390MPa and elongation of more than 12%. The effect of adding three microalloying elements is very obvious, and Zr can effectively refine grains; nd can refine the as-cast structure, change the deformation mechanism and improve the toughness of the alloy; the Sr function is mainly embodied in refining and deteriorating the structure of the magnesium alloy, and solid solution strengthening is generated. The higher extrusion ratio enables the volume fraction of new crystal grains to be larger in the deformation process, and dynamic recrystallization can be repeatedly carried out under certain conditions, so that the crystal grains are obviously refined, and the average crystal grain size is 3-5 mu m. After the later-stage solid solution and aging treatment, a large amount of nano dispersion strengthening phases are separated out, and finally, the comprehensive mechanical property and the processing property of the alloy are obviously improved and enhanced.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
the raw materials were proportioned and weighed according to the designed alloy composition Mg-8Al-0.3Zn-0.3Mn-0.3Zr-0.2Nd-0.1Sr (wt.%) (each 1000g of target alloy consists of 80gAl, 3gZn, 1gSr, 10gMg-30Zr master alloy, 20gMg-10Nd master alloy, 6.9gMnCl2 and 879.1g of pure magnesium blocks). The preparation method comprises the following specific steps:
(1) the method is characterized in that a steel crucible is adopted, the steel crucible is heated to 200 ℃ after being cleaned, the surface of the steel crucible is coated with mixed liquid of talcum powder, water glass and water for three times, and then the mixed liquid of ZnO, water glass and water is coated for three times. Until the surface of the steel crucible is not exposed to avoid the pollution of Fe element. After each coating, the crucible is placed back into the heating furnace for heat preservation for 20 minutes;
(2) preheating the coated crucible to 520 ℃, putting the magnesium block preheated to 200 ℃ into the crucible, and scattering a covering agent on the surface of the magnesium block. Then introducing argon to the opening of the crucible for gas protection, heating to 700 ℃, and preserving heat for 30 minutes to wait for the magnesium block to be melted into a bulk state;
(3) after the magnesium block is melted, rapidly removing slag according to the oxidation and impurity conditions on the surface of the solution, then sequentially adding alloying elements such as pure zinc, pure aluminum, pure strontium, Mg-Zr intermediate alloy, Mg-Nd intermediate alloy and MnCl2 particles into the magnesium alloy solution according to the mixture ratio of the raw materials, fully stirring, uniformly scattering a covering agent on the surface of the solution after stirring, and preserving heat for 30 minutes at 700 ℃;
(4) after heat preservation, the furnace temperature is raised to 730 ℃ for refining, a refining agent with the total weight fraction of 1.5 percent is added into the solution, the mixture is fully stirred for 10 minutes and then is preserved for 30 minutes at 730 ℃;
(5) cooling the furnace to 680 ℃ after heat preservation, and pouring the furnace into a metal mold which is preserved at 200 ℃ in advance for cooling and solidification;
(6) carrying out homogenizing annealing on the magnesium alloy ingot at 400 ℃, keeping the temperature for 12 hours, machining the blank into a required size after homogenizing annealing, and peeling;
(7) preheating the machined blank to 420 ℃, putting the blank on an extruder for extrusion forming, wherein the preheating temperature of an extrusion cylinder is 400 ℃, the extrusion temperature is 440 ℃, the extrusion ratio is 25:1, the extrusion speed is 3.5m/min, and the obtained section bar is cooled to room temperature by air;
(8) the obtained magnesium alloy section is subjected to solution treatment for 2 hours at 380 ℃ and aging treatment for 18 hours at 170 ℃, and finally the high-strength and high-toughness magnesium alloy section is prepared.
Example 2:
the raw materials are proportioned and weighed according to the designed alloy components Mg-7Al-0.6Zn-0.15Mn-0.6Zr-0.5Nd-0.3Sr (wt.%) (each 1000g of target alloy consists of 70g of Al, 6gZn, 3gSr, 20g of Mg-30Zr intermediate alloy, 50g of Mg-10Nd intermediate alloy, 3.45g of MnCl2 and 847.55g of pure magnesium blocks). The preparation method comprises the following specific steps:
(1) the method is characterized in that a steel crucible is adopted, the steel crucible is heated to 200 ℃ after being cleaned, the surface of the steel crucible is coated with mixed liquid of talcum powder, water glass and water for three times, and then the mixed liquid of ZnO, water glass and water is coated for three times. Until the surface of the steel crucible is not exposed to avoid the pollution of Fe element. After each coating, the crucible is placed back into the heating furnace for heat preservation for 20 minutes;
(2) preheating the coated crucible to 520 ℃, putting the magnesium block preheated to 200 ℃ into the crucible, and scattering a covering agent on the surface of the magnesium block. Then introducing argon to the opening of the crucible for gas protection, heating to 700 ℃, and preserving heat for 30 minutes to wait for the magnesium block to be melted into a bulk state;
(3) after the magnesium block is melted, rapidly removing slag according to the oxidation and impurity conditions on the surface of the solution, then sequentially adding alloying elements such as pure zinc, pure aluminum, pure strontium, Mg-Zr intermediate alloy, Mg-Nd intermediate alloy and MnCl2 particles into the magnesium alloy solution according to the mixture ratio of the raw materials, fully stirring, uniformly scattering a covering agent on the surface of the solution after stirring, and preserving heat for 30 minutes at 700 ℃;
(4) after heat preservation, the furnace temperature is raised to 730 ℃ for refining, a refining agent with the total weight fraction of 1.5 percent is added into the solution, the mixture is fully stirred for 10 minutes and then is preserved for 30 minutes at 730 ℃;
(5) cooling the furnace to 680 ℃ after heat preservation, and pouring the furnace into a metal mold which is preserved at 200 ℃ in advance for cooling and solidification;
(6) carrying out homogenizing annealing on the cast magnesium alloy ingot at 400 ℃, keeping the temperature for 12 hours, machining the blank into a required size after homogenizing annealing, and peeling;
(7) preheating the machined blank to 420 ℃, putting the blank on an extruder for extrusion forming, wherein the preheating temperature of an extrusion cylinder is 400 ℃, the extrusion temperature is 440 ℃, the extrusion ratio is 25:1, the extrusion speed is 3.5m/min, and the obtained section bar is cooled to room temperature by air;
(8) the obtained magnesium alloy section is subjected to solution treatment for 2 hours at 380 ℃ and aging treatment for 18 hours at 170 ℃, and finally the high-strength and high-toughness magnesium alloy section is prepared.
Example 3:
the raw materials are proportioned and weighed according to the designed alloy components Mg-9Al-0.8Zn-0.5Mn-0.9Zr-0.1Nd-0.5Sr (wt.%) (each 1000g of target alloy consists of 90g of Al, 8gZn, 5gSr, 30g of Mg-30Zr intermediate alloy, 10g of Mg-10Nd intermediate alloy, 11.5g of MnCl2 and 845.5g of pure magnesium blocks). The preparation method comprises the following specific steps:
(1) the method is characterized in that a steel crucible is adopted, the steel crucible is heated to 200 ℃ after being cleaned, the surface of the steel crucible is coated with mixed liquid of talcum powder, water glass and water for three times, and then the mixed liquid of ZnO, water glass and water is coated for three times. Until the surface of the steel crucible is not exposed to avoid the pollution of Fe element. After each coating, the crucible is placed back into the heating furnace for heat preservation for 20 minutes;
(2) preheating the coated crucible to 520 ℃, putting the magnesium block preheated to 200 ℃ into the crucible, and scattering a covering agent on the surface of the magnesium block. Then introducing argon to the opening of the crucible for gas protection, heating to 700 ℃, and preserving heat for 30 minutes to wait for the magnesium block to be melted into a bulk state;
(3) after the magnesium block is melted, rapidly removing slag according to the oxidation and impurity conditions on the surface of the solution, then sequentially adding alloying elements such as pure zinc, pure aluminum, pure strontium, Mg-Zr intermediate alloy, Mg-Nd intermediate alloy and MnCl2 particles into the magnesium alloy solution according to the mixture ratio of the raw materials, fully stirring, uniformly scattering a covering agent on the surface of the solution after stirring, and preserving heat for 30 minutes at 700 ℃;
(4) after heat preservation, the furnace temperature is raised to 730 ℃ for refining, a refining agent with the total weight fraction of 1.5 percent is added into the solution, the mixture is fully stirred for 10 minutes and then is preserved for 30 minutes at 730 ℃;
(5) cooling the furnace to 680 ℃ after heat preservation, and pouring the furnace into a metal mold which is preserved at 200 ℃ in advance for cooling and solidification;
(6) carrying out homogenizing annealing on the cast magnesium alloy ingot at 400 ℃, keeping the temperature for 12 hours, machining the blank into a required size after homogenizing annealing, and peeling;
(7) preheating the machined blank to 420 ℃, putting the blank on an extruder for extrusion forming, wherein the preheating temperature of an extrusion cylinder is 400 ℃, the extrusion temperature is 440 ℃, the extrusion ratio is 25:1, the extrusion speed is 3.5m/min, and the obtained section bar is cooled to room temperature by air;
(8) the obtained magnesium alloy section is subjected to solution treatment for 2 hours at 380 ℃ and aging treatment for 18 hours at 170 ℃, and finally the high-strength and high-toughness magnesium alloy section is prepared.
Mechanical property parameters of magnesium alloy section bar at room temperature prepared by three embodiments
| Examples | Yield strength (MPa) | Tensile strength (MPa) | Elongation (%) |
| Example 1 | 284 | 390 | 12.2 |
| Example 2 | 289 | 391 | 12.8 |
| Example 3 | 292 | 398 | 12.6 |
The high-strength and high-toughness wrought magnesium alloy prepared by the composite treatment method has the beneficial effects that the high-strength and high-toughness wrought magnesium alloy has higher strength and good ductility, the comprehensive mechanical property and the processing property of AZ80 are further improved and improved, the yield strength is more than 280MPa, the tensile strength is more than 390MPa, and the elongation is more than 12%. The effect of adding three microalloying elements is very obvious, and Zr can effectively refine grains; nd can refine the as-cast structure, change the deformation mechanism and improve the toughness of the alloy; the Sr function is mainly embodied in refining and deteriorating the structure of the magnesium alloy, and solid solution strengthening is generated. The higher extrusion ratio enables the volume fraction of new crystal grains to be larger in the deformation process, and dynamic recrystallization can be repeatedly carried out under certain conditions, so that the crystal grains are obviously refined, and the average crystal grain size is 3-5 mu m. After the later-stage solid solution and aging treatment, a large amount of nano dispersion strengthening phases are separated out, and finally, the comprehensive mechanical property and the processing property of the alloy are obviously improved and enhanced.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. The high-strength and high-toughness wrought magnesium alloy is characterized in that microalloying elements of Zr, Nd and Sr are added to a commonly used AZ80 magnesium alloy through a composite treatment method, and the high-strength and high-toughness wrought magnesium alloy is characterized in that the alloy comprises the following components in percentage by weight: 7.8 to 9.2 percent of All, 0.2 to 0.8 percent of Zn0.15 to 0.5 percent of Mn0.3 to 1 percent of Zr0.3 to 1 percent of Nd0.1 to 0.5 percent of Sr0.1 to 0.5 percent of impurity elements, wherein the impurity elements are Si, Fe, Ni and Cu, the total content is less than 0.08 percent, and the balance is Mg;
the preparation method of the high-strength and high-toughness wrought magnesium alloy comprises the following steps of:
(1) taking a steel crucible, cleaning the steel crucible, heating the steel crucible to 200 ℃, painting a mixed solution of talcum powder, water glass and water for three times on the surface of the steel crucible, painting a mixed solution of ZnO, water glass and water for three times after the cleaning is finished until the surface of the steel crucible is not exposed, and putting the steel crucible back into a heating furnace for heat preservation for 20 minutes after each painting;
(2) preheating a coated crucible to 520 ℃, putting a magnesium block preheated to 200 ℃, scattering a covering agent on the surface of the magnesium block, then introducing argon to the opening of the crucible, heating the crucible to 700 ℃, preserving the temperature for 30 minutes, and waiting for the magnesium block to be melted into a liquid state;
(3) after the magnesium block is melted, rapidly removing slag according to the oxidation and impurity conditions on the surface of the solution, and then adding pure zinc, pure aluminum, pure strontium, Mg-Zr intermediate alloy, Mg-Nd intermediate alloy and MnCl2Sequentially adding the particles into the magnesium alloy solution, fully stirring, uniformly scattering a covering agent on the surface of the solution after stirring, and preserving heat for 30 minutes at 700 ℃;
(4) after heat preservation, the furnace temperature is increased to 730 ℃ for refining, a refining agent with the total weight percentage of 1.5% is added into the solution, and after full stirring for 10 minutes, heat preservation is carried out for 30 minutes at 730 ℃;
(5) reducing the furnace temperature to 680 ℃ after heat preservation, and pouring the furnace temperature into a metal mold preserved at 200 ℃ in advance for cooling and solidification;
(6) homogenizing annealing magnesium alloy ingots at 400 ℃, keeping the temperature for 12 hours, machining blanks into required sizes after homogenizing annealing, and peeling;
(7) preheating the machined blank to 420 ℃, putting the blank on an extruder for extrusion forming, wherein the preheating temperature of an extrusion cylinder is 400 ℃, the extrusion temperature is 440 ℃, and the extrusion ratio is 25:1, extruding at the speed of 3.5m/min, and cooling the obtained section bar to room temperature in air;
(8) the obtained magnesium alloy section is subjected to solution treatment for 2 hours at 380 ℃ and aging treatment for 18 hours at 170 ℃, and finally the high-strength and high-toughness magnesium alloy section is prepared.
2. The high-strength high-toughness wrought magnesium alloy according to claim 1, wherein: the raw material purity in the step (3) is 99.9% of pure magnesium blocks, 99.9% of pure zinc blocks, 99.9% of pure aluminum blocks, 99.9% of pure strontium blocks and 99.9% of MnCl 2.
3. The high-strength high-toughness wrought magnesium alloy according to claim 1, wherein: the mixed liquid of the talcum powder, the water glass and the water used in the step (1) comprises the following components in a volume ratio of 25: 6: 69.
4. the high-strength high-toughness wrought magnesium alloy according to claim 1, wherein: the volume ratio of the components of the mixed liquid of ZnO, water glass and water used in the step (1) is 22: 6: 72.
5. the high-strength high-toughness wrought magnesium alloy according to claim 1, wherein: the covering agent used in the step (2) and the step (3) comprises the following components in percentage by weight: CaCl2：BaCl2：NaCl=52：28：17：3。
6. The high-strength high-toughness wrought magnesium alloy according to claim 1, wherein: the refining agent used in the step (4) comprises the following components in percentage by weight: CaCl2：BaCl2：NaCl：CaF2=50：27：16：2：5。
7. The high-strength high-toughness wrought magnesium alloy according to claim 1, wherein: MnCl used in the step (3)2Is granular with a diameter of 1-3 mm.
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| CN110624969A (en) * | 2019-11-08 | 2019-12-31 | 兰州理工大学 | Extrusion deformation device for preparing high-strength magnesium alloy and preparation method |
| CN111020253B (en) * | 2019-11-14 | 2021-11-16 | 李健 | Biomedical magnesium alloy processing method |
| CN111112551B (en) * | 2020-01-14 | 2021-03-09 | 山西神舟航天科技有限公司 | Forming method of large-size magnesium alloy casting |
| CN112746210B (en) * | 2021-02-01 | 2021-10-12 | 太原理工大学 | Multi-element microalloyed magnesium alloy, preparation method thereof and plate extrusion forming process |
| CN112746189B (en) * | 2021-02-01 | 2021-09-24 | 太原理工大学 | Preparation method of high-toughness magnesium alloy and roll forming process of plate thereof |
| CN114231777B (en) * | 2021-12-13 | 2022-12-13 | 上海航天精密机械研究所 | Bromine-containing refining agent for rapid sedimentation rare earth magnesium alloy, preparation method and application |
| CN115572874B (en) * | 2022-11-15 | 2023-11-07 | 中北大学 | Preparation method of high-conductivity Mg-Zn-Cu magnesium alloy |
| CN116240416A (en) * | 2022-12-14 | 2023-06-09 | 上海航天精密机械研究所 | Low-foam low-smoke refining agent for rare earth magnesium alloy and preparation method thereof |
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